CN108311144A - A kind of dumbbell shaped nanogold-platinum composite catalyst and preparation method thereof - Google Patents
A kind of dumbbell shaped nanogold-platinum composite catalyst and preparation method thereof Download PDFInfo
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- CN108311144A CN108311144A CN201810009155.XA CN201810009155A CN108311144A CN 108311144 A CN108311144 A CN 108311144A CN 201810009155 A CN201810009155 A CN 201810009155A CN 108311144 A CN108311144 A CN 108311144A
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- 239000003054 catalyst Substances 0.000 title claims abstract description 32
- BASFCYQUMIYNBI-UHFFFAOYSA-N platinum Substances [Pt] BASFCYQUMIYNBI-UHFFFAOYSA-N 0.000 title claims abstract description 23
- 229910052697 platinum Inorganic materials 0.000 title claims abstract description 21
- 238000002360 preparation method Methods 0.000 title claims abstract description 20
- 239000002131 composite material Substances 0.000 title claims abstract description 19
- SQGYOTSLMSWVJD-UHFFFAOYSA-N silver(1+) nitrate Chemical compound [Ag+].[O-]N(=O)=O SQGYOTSLMSWVJD-UHFFFAOYSA-N 0.000 claims abstract description 39
- CIWBSHSKHKDKBQ-JLAZNSOCSA-N Ascorbic acid Chemical compound OC[C@H](O)[C@H]1OC(=O)C(O)=C1O CIWBSHSKHKDKBQ-JLAZNSOCSA-N 0.000 claims abstract description 24
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims abstract description 20
- 229960005070 ascorbic acid Drugs 0.000 claims abstract description 12
- 239000002253 acid Substances 0.000 claims abstract description 11
- 235000010323 ascorbic acid Nutrition 0.000 claims abstract description 11
- 239000011668 ascorbic acid Substances 0.000 claims abstract description 11
- PCHJSUWPFVWCPO-UHFFFAOYSA-N gold Chemical compound [Au] PCHJSUWPFVWCPO-UHFFFAOYSA-N 0.000 claims abstract description 10
- 229910001961 silver nitrate Inorganic materials 0.000 claims abstract description 10
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical class O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 claims abstract description 7
- 239000000203 mixture Substances 0.000 claims abstract description 5
- QKXCAKZMAORNSR-UHFFFAOYSA-N azane 1-chlorohexadecane Chemical compound N.CCCCCCCCCCCCCCCCCl QKXCAKZMAORNSR-UHFFFAOYSA-N 0.000 claims abstract description 4
- RJHLTVSLYWWTEF-UHFFFAOYSA-K gold trichloride Chemical class Cl[Au](Cl)Cl RJHLTVSLYWWTEF-UHFFFAOYSA-K 0.000 claims abstract description 4
- XQSBLCWFZRTIEO-UHFFFAOYSA-N hexadecan-1-amine;hydrobromide Chemical compound [Br-].CCCCCCCCCCCCCCCC[NH3+] XQSBLCWFZRTIEO-UHFFFAOYSA-N 0.000 claims abstract description 4
- 230000036571 hydration Effects 0.000 claims abstract description 4
- 238000006703 hydration reaction Methods 0.000 claims abstract description 4
- -1 enuatrol Chemical compound 0.000 claims abstract 2
- 239000000243 solution Substances 0.000 claims description 52
- 238000003756 stirring Methods 0.000 claims description 13
- 229910003603 H2PdCl4 Inorganic materials 0.000 claims description 10
- 229910004042 HAuCl4 Inorganic materials 0.000 claims description 9
- 229910017604 nitric acid Inorganic materials 0.000 claims description 9
- 229910000033 sodium borohydride Inorganic materials 0.000 claims description 9
- 239000012279 sodium borohydride Substances 0.000 claims description 9
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 8
- 229910021642 ultra pure water Inorganic materials 0.000 claims description 7
- 239000012498 ultrapure water Substances 0.000 claims description 7
- LZZYPRNAOMGNLH-UHFFFAOYSA-M Cetrimonium bromide Chemical compound [Br-].CCCCCCCCCCCCCCCC[N+](C)(C)C LZZYPRNAOMGNLH-UHFFFAOYSA-M 0.000 claims description 6
- 229910002621 H2PtCl6 Inorganic materials 0.000 claims description 6
- 150000007513 acids Chemical class 0.000 claims description 6
- WOWHHFRSBJGXCM-UHFFFAOYSA-M cetyltrimethylammonium chloride Chemical compound [Cl-].CCCCCCCCCCCCCCCC[N+](C)(C)C WOWHHFRSBJGXCM-UHFFFAOYSA-M 0.000 claims description 6
- NICDRCVJGXLKSF-UHFFFAOYSA-N nitric acid;trihydrochloride Chemical compound Cl.Cl.Cl.O[N+]([O-])=O NICDRCVJGXLKSF-UHFFFAOYSA-N 0.000 claims description 6
- 238000006243 chemical reaction Methods 0.000 claims description 4
- 239000011521 glass Substances 0.000 claims description 3
- 239000011259 mixed solution Substances 0.000 claims description 3
- 238000005119 centrifugation Methods 0.000 claims description 2
- QYSYEILYXGRUOM-UHFFFAOYSA-N [Cl].[Pt] Chemical compound [Cl].[Pt] QYSYEILYXGRUOM-UHFFFAOYSA-N 0.000 claims 1
- 239000007788 liquid Substances 0.000 claims 1
- 229940088594 vitamin Drugs 0.000 claims 1
- 229930003231 vitamin Natural products 0.000 claims 1
- 235000013343 vitamin Nutrition 0.000 claims 1
- 239000011782 vitamin Substances 0.000 claims 1
- 150000003722 vitamin derivatives Chemical class 0.000 claims 1
- 230000003197 catalytic effect Effects 0.000 abstract description 12
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 abstract description 6
- 239000001301 oxygen Substances 0.000 abstract description 6
- 229910052760 oxygen Inorganic materials 0.000 abstract description 6
- 238000006555 catalytic reaction Methods 0.000 abstract description 4
- 239000000975 dye Substances 0.000 abstract description 4
- 239000010842 industrial wastewater Substances 0.000 abstract description 3
- 239000002245 particle Substances 0.000 abstract description 3
- 239000010931 gold Substances 0.000 abstract description 2
- 239000002105 nanoparticle Substances 0.000 abstract description 2
- 230000009467 reduction Effects 0.000 abstract description 2
- 239000002699 waste material Substances 0.000 abstract description 2
- 238000004065 wastewater treatment Methods 0.000 abstract description 2
- KEAYESYHFKHZAL-UHFFFAOYSA-N Sodium Chemical compound [Na] KEAYESYHFKHZAL-UHFFFAOYSA-N 0.000 abstract 1
- 229910052737 gold Inorganic materials 0.000 abstract 1
- 229910000104 sodium hydride Inorganic materials 0.000 abstract 1
- 239000012312 sodium hydride Substances 0.000 abstract 1
- KDLHZDBZIXYQEI-UHFFFAOYSA-N Palladium Chemical compound [Pd] KDLHZDBZIXYQEI-UHFFFAOYSA-N 0.000 description 14
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 8
- GQDHEYWVLBJKBA-UHFFFAOYSA-H copper(ii) phosphate Chemical compound [Cu+2].[Cu+2].[Cu+2].[O-]P([O-])([O-])=O.[O-]P([O-])([O-])=O GQDHEYWVLBJKBA-UHFFFAOYSA-H 0.000 description 6
- GDSOZVZXVXTJMI-SNAWJCMRSA-N (e)-1-methylbut-1-ene-1,2,4-tricarboxylic acid Chemical compound OC(=O)C(/C)=C(C(O)=O)\CCC(O)=O GDSOZVZXVXTJMI-SNAWJCMRSA-N 0.000 description 4
- 230000000694 effects Effects 0.000 description 4
- 229910052757 nitrogen Inorganic materials 0.000 description 4
- 239000000126 substance Substances 0.000 description 4
- 239000002351 wastewater Substances 0.000 description 4
- UHOVQNZJYSORNB-UHFFFAOYSA-N Benzene Chemical compound C1=CC=CC=C1 UHOVQNZJYSORNB-UHFFFAOYSA-N 0.000 description 3
- 230000003647 oxidation Effects 0.000 description 3
- 238000007254 oxidation reaction Methods 0.000 description 3
- 238000005406 washing Methods 0.000 description 3
- BTJIUGUIPKRLHP-UHFFFAOYSA-N 4-nitrophenol Chemical compound OC1=CC=C([N+]([O-])=O)C=C1 BTJIUGUIPKRLHP-UHFFFAOYSA-N 0.000 description 2
- 230000010718 Oxidation Activity Effects 0.000 description 2
- ISWSIDIOOBJBQZ-UHFFFAOYSA-N Phenol Chemical compound OC1=CC=CC=C1 ISWSIDIOOBJBQZ-UHFFFAOYSA-N 0.000 description 2
- NBIIXXVUZAFLBC-UHFFFAOYSA-N Phosphoric acid Chemical compound OP(O)(O)=O NBIIXXVUZAFLBC-UHFFFAOYSA-N 0.000 description 2
- 238000002484 cyclic voltammetry Methods 0.000 description 2
- 239000003792 electrolyte Substances 0.000 description 2
- 238000000034 method Methods 0.000 description 2
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 description 1
- 239000012028 Fenton's reagent Substances 0.000 description 1
- DGAQECJNVWCQMB-PUAWFVPOSA-M Ilexoside XXIX Chemical compound C[C@@H]1CC[C@@]2(CC[C@@]3(C(=CC[C@H]4[C@]3(CC[C@@H]5[C@@]4(CC[C@@H](C5(C)C)OS(=O)(=O)[O-])C)C)[C@@H]2[C@]1(C)O)C)C(=O)O[C@H]6[C@@H]([C@H]([C@@H]([C@H](O6)CO)O)O)O.[Na+] DGAQECJNVWCQMB-PUAWFVPOSA-M 0.000 description 1
- 239000002211 L-ascorbic acid Substances 0.000 description 1
- 235000000069 L-ascorbic acid Nutrition 0.000 description 1
- 230000004075 alteration Effects 0.000 description 1
- 229910000147 aluminium phosphate Inorganic materials 0.000 description 1
- 238000004458 analytical method Methods 0.000 description 1
- 230000008901 benefit Effects 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 230000015556 catabolic process Effects 0.000 description 1
- 230000008859 change Effects 0.000 description 1
- 239000003795 chemical substances by application Substances 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 229910052802 copper Inorganic materials 0.000 description 1
- 239000010949 copper Substances 0.000 description 1
- 230000007812 deficiency Effects 0.000 description 1
- 238000006731 degradation reaction Methods 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 238000003912 environmental pollution Methods 0.000 description 1
- 238000006197 hydroboration reaction Methods 0.000 description 1
- 230000006872 improvement Effects 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 229910052763 palladium Inorganic materials 0.000 description 1
- 230000008569 process Effects 0.000 description 1
- 238000012545 processing Methods 0.000 description 1
- 238000006479 redox reaction Methods 0.000 description 1
- 230000001603 reducing effect Effects 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 229910052708 sodium Inorganic materials 0.000 description 1
- 239000011734 sodium Substances 0.000 description 1
- 238000003786 synthesis reaction Methods 0.000 description 1
- 238000010189 synthetic method Methods 0.000 description 1
- 239000003643 water by type Substances 0.000 description 1
- 238000009279 wet oxidation reaction Methods 0.000 description 1
Classifications
-
- B01J35/393—
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J23/00—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00
- B01J23/38—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of noble metals
- B01J23/48—Silver or gold
- B01J23/52—Gold
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J35/00—Catalysts, in general, characterised by their form or physical properties
-
- B01J35/30—
-
- B01J35/396—
Abstract
The invention discloses a kind of dumbbell shaped nanogold platinum composite catalysts, it is characterised in that：It is used in preparation process including compositions such as cetyl chloride ammonium, enuatrol, sodium hydride, cetyl ammonium bromide, three hydration gold chlorides, silver nitrate, ascorbic acid, chloroplatinic acid, concentrated hydrochloric acid and concentrated nitric acids, and is prepared for the composite catalyst with special appearance：Dumbbell shaped nanogold platinum composite catalyst, the main anchor of nano-platinum particle close at the both ends of nanometer gold bar, and dumbbell shaped is presented in composite nanoparticle monnolithic case.Its catalysis characteristics is applied to wastewater treatment, solves the problems, such as that catalyst in the prior art is not ideal enough to the dyestuff the like waste catalytic effect in industrial wastewater, there is preferable oxygen reduction catalytic activity.
Description
Technical field
The invention belongs to chemical catalyst technical fields, more particularly to a kind of dumbbell shaped nanogold-platinum composite catalyst
And preparation method thereof.
Background technology
With the development of chemical industry, environmental pollution getting worse.Wherein, the discharge capacity of the waste water from dyestuff in industrial wastewater
It is big and difficult, it is always the Major Difficulties of wastewater treatment.Wet oxidation is the important side for handling such waste water from dyestuff difficult to degrade
Method.Heterogeneous catalytic oxidation under temperate condition has more traditional Fenton reagent unique advantage and is taken seriously, Cheap highly effective catalysis
Agent exploitation is the key that the treatment process.Xiao Fengshou etc. ((F.S.Xiaoe seven alJCata1.2001,199:273-281) first
It was found that synthesis is a kind of new catalytic material with applications well foreground through base cupric phosphate, in a mild condition a series of
Excellent catalytic performance is shown during green oxidation.For example, through base cupric phosphate in catalysis through changing the side such as benzene, phenol and Cai's phenol
Face superior performance.The catalytic activity of light base cupric phosphate is better than famous silicalite TS-1 of admiring.But since oxidation activity is excessively high, easily
Tar is generated in deep oxidation, limits its application.The characteristics of in order to play the catalyst high oxidation activity, also through base cupric phosphate
It is used for the degradation treatment of p-nitrophenol waste water, and achieves better effects.(the Chemical Journal of Chinese Universities such as Wang Runwei
20081331-1333) report the quick light base cupric phosphate of green syt under hydrothermal condition.Recently, Zhou Xiang (Zhengzhou University 2010)
The preparation of the light base cupric phosphate of stratiform is reported, the treatment effect for high concentrated organic wastewater is apparent.Therefore seek light base phosphoric acid
The synthetic method of copper simplicity becomes the emphasis of catalyticing research with its catalytic activity is improved.
Invention content
The purpose of the present invention is being directed to deficiency in the prior art, a kind of dumbbell shaped nanogold-platinum composite catalyst is provided
And preparation method thereof, it solves catalyst in the prior art and dyestuff the like waste catalytic effect in industrial wastewater is not enough managed
The problem of thinking.
In order to achieve the above object, there is provided a kind of dumbbell shaped nanogold-platinum is compound for the technical solution adopted by the present invention
Catalyst, including cetyl chloride ammonium, enuatrol, chloroplatinic acid, sodium borohydride, cetyl ammonium bromide, three hydration gold chlorides,
Silver nitrate, ascorbic acid, concentrated hydrochloric acid and concentrated nitric acid.
Preferably, each component concentration is as follows
CTAC97%
NaOL97%
H2PtCl6·6H2O98%
NaBH499%
CTAB98%
HAuCl4·3H2O99.99%
AgNO399.99%
AA>99.5%
HCl36.0~37.0%
HNO365.0~68.0%.
The present invention also provides a kind of preparation methods of dumbbell shaped nanogold-platinum composite catalyst, comprise the following steps：
S1：Glass reaction container is impregnated into 12h in chloroazotic acid；
S2：CTAB is added in measuring cup, HAuCl is then added410~20min of solution ＆ stir is added fresh
The NaBH of preparation4Solution is vigorously stirred 2min, and solution colour becomes brown color from yellow, after standing 30min under the conditions of 30 DEG C
It is spare；
S3：Weigh CTAB7.0g, NaOL1.234g, H2PtCl6·6H2O1.2g is placed in 500mL conical flasks, and is added
250mL, 55 DEG C of ultra-pure water wait for that solution is cooled to 30 DEG C, AgNO3 solution are added, and stand 15min under the conditions of 30 DEG C；With
After HAuCl is added4Solution, stirs 90min at 700r/min, and solution is become colorless by yellow；HCl is added, in 400r/min
Stir 15min；Then ascorbic acid is added in the mixed solution and is vigorously stirred 30s；0.4mL seed-solutions are finally taken to add
Enter into growth solution, after being vigorously stirred 30s, 30 DEG C of standing 12h obtain gold nanorods stoste, and gold nanorods stoste centrifuges simultaneously
Twice, gained gold nanorods are dispersed in 0.1mol/L50mLCTAC solution, are stored in spare in 35 DEG C of baking oven for washing；
S4：By AA and H2PdCl4 according to the ratio between mole, sample is prepared, steps are as follows:Take the AuNRs of CTAC modifieds
Solution 2mL is placed in 40mL measuring cups, is diluted with water to 20mL；3mL, 0.01mol/L chloroplatinic acids and 4mL, 1mmol/L is added
Silver nitrate adds 0.05mmol/L ascorbic acid, and 30s is stirred at 700r/min, then 30 DEG C of standing 12h, product centrifugation
Processing washing twice, is finally dispersed in 5mL ultra-pure waters.
As a kind of improvement of this programme, the volume that ascorbic acid is added in S4 is 60 μ L, 150 μ L, 600 μ L or 300 μ L.
Preferably, it is 3 that the chloroazotic acid described in S1, which is concentrated hydrochloric acid with concentrated nitric acid according to volume ratio,:The solution of 1 composition.
Preferably, the CTAB amounts described in S2 are 0.2mol/L, 5mL；HAuCl4Solution is 0.5mmol/L, 5mL；NaBH4
Solution is 6mmol/L, 1mL.
Preferably, the AgNO3 solution described in S3 is 4mmol/L, 24mL；HAuCl4Solution is 1mmol/L, 250mL；
HCl amounts are 37wt%, 4.8mL；Ascorbic acid is 64mmol/L, 1.25mL.
Compared with prior art, the catalyst of the application shows good catalysis p-nitrophenol reducing property, urges
Change activity mainly to be determined in the dispersibility at golden stick both ends and total active site by nano-platinum particle.With nano-platinum particle ruler
The very little Au/PdNDs (0.04mg/mL) for 20.7nm is used as catalyst, and reaction rate constant is up to 0.44min-1, than most of
The catalytic activity of supported palladium catalyst will be high, it was demonstrated that it is a kind of very effective catalyst.
Description of the drawings
Fig. 1 is cyclic voltammetry curve of the catalyst in nitrogen and oxygen of the present invention
Fig. 2 is LSV curve of the catalyst of the present invention under nitrogen and oxygen different rotating speeds
Specific implementation mode
Form below by specific embodiment be to be described in detail to technical scheme of the present invention is further, but
Following embodiment only plays the effect for helping to understand the present invention, can not be not understood as limitation of the invention further.
A kind of dumbbell shaped nanogold-platinum composite catalyst, including cetyl chloride ammonium, enuatrol, chloroplatinic acid, hydroboration
Sodium, cetyl ammonium bromide, three hydration gold chlorides, silver nitrate, ascorbic acid, concentrated hydrochloric acid and concentrated nitric acid.
Preferably, each component concentration is as follows
CTAC97%
NaOL97%
H2PtCl6·6H2O98%
NaBH499%
CTAB98%
HAuCl4·3H2O99.99%
AgNO399.99%
AA>99.5%
HCl36.0~37.0%
HNO365.0~68.0%.
Embodiment one：A kind of preparation method of dumbbell shaped nanogold-platinum composite catalyst, comprises the following steps：
S1：Glass reaction container is impregnated into 12h in chloroazotic acid；
S2：CTAB is added in measuring cup, HAuCl is then added410~20min of solution ＆ stir is added fresh
The NaBH of preparation4Solution is vigorously stirred 2min, and solution colour becomes brown color from yellow, after standing 30min under the conditions of 30 DEG C
It is spare；
S3：Weigh CTAB7.0g, NaOL1.234g, H2PtCl6·6H2O1.2g is placed in 500mL conical flasks, and is added
250mL, 55 DEG C of ultra-pure water wait for that solution is cooled to 30 DEG C, AgNO3 solution are added, and stand 15min under the conditions of 30 DEG C；With
After HAuCl is added4Solution, stirs 90min at 700r/min, and solution is become colorless by yellow；HCl is added, in 400r/min
Stir 15min；Then ascorbic acid is added in the mixed solution and is vigorously stirred 30s；0.4mL seed-solutions are finally taken to add
Enter into growth solution, after being vigorously stirred 30s, 30 DEG C of standing 12h obtain gold nanorods stoste, and gold nanorods stoste centrifuges simultaneously
Twice, gained gold nanorods are dispersed in 0.1mol/L50mLCTAC solution, are stored in spare in 35 DEG C of baking oven for washing；
S4：The ratio between the mole for changing AA and H2PdCl4, is prepared for AA:H2PdCl4=0.1 sample, and be labeled as
AA:Pd=0.1.
Sample AA:The preparation process of Pd=0.1 is as follows:
It takes the AuNRs solution 2mL of CTAC modifieds to be placed in 40mL measuring cups, is diluted with water to 20mL；
It is firstly added 3mL0.01mol/L chloroplatinic acids and 4mL1mmol/L silver nitrates, it is anti-bad to add 60 μ L0.05mmol/L
Hematic acid stirs 30s at 700r/min, and then 30 DEG C of standing 12h, product centrifugal treating are washed twice, are finally dispersed in 5mL
In ultra-pure water.
It is 3 that chloroazotic acid described in S1, which is concentrated hydrochloric acid with concentrated nitric acid according to volume ratio,:The solution of 1 composition.
CTAB amounts described in S2 are 0.2mol/L, 5mL；HAuCl4Solution is 0.5mmol/L, 5mL；NaBH4Solution is
6mmol/L, 1mL.
AgNO3 solution described in S3 is 4mmol/L, 24mL；HAuCl4Solution is 1mmol/L, 250mL；HCl amounts are
37wt%, 4.8mL；Ascorbic acid is 64mmol/L, 1.25mL.
Embodiment two：Embodiments thereof and embodiment one are essentially identical, the difference is that：
S4：The ratio between the mole for changing AA and H2PdCl4, is prepared for AA:H2PdCl4=0.25 sample, and be labeled as
AA:Pd=0.25.
Sample AA:The preparation process of Pd=0.25 is as follows:
It takes the AuNRs solution 2mL of CTAC modifieds to be placed in 40mL measuring cups, is diluted with water to 20mL；
It is firstly added 3mL0.01mol/L chloroplatinic acids and 4mL1mmol/L silver nitrates, it is anti-to add 150 μ L0.05mmol/L
Bad hematic acid stirs 30s at 700r/min, and then 30 DEG C of standing 12h, product centrifugal treating are washed twice, are finally dispersed in 5mL
In ultra-pure water.
Embodiment three：Embodiments thereof and embodiment one are essentially identical, the difference is that：
S4：The ratio between the mole for changing AA and H2PdCl4, is prepared for AA:H2PdCl4=0.5 sample, and be labeled as
AA:Pd=0.5.
Sample AA:The preparation process of Pd=0.5 is as follows:
It takes the AuNRs solution 2mL of CTAC modifieds to be placed in 40mL measuring cups, is diluted with water to 20mL；
It is firstly added 3mL0.01mol/L chloroplatinic acids and 4mL1mmol/L silver nitrates, it is anti-to add 300 μ L0.05mmol/L
Bad hematic acid stirs 30s at 700r/min, and then 30 DEG C of standing 12h, product centrifugal treating are washed twice, are finally dispersed in 5mL
In ultra-pure water；
Example IV：Embodiments thereof and embodiment one are essentially identical, the difference is that：
S4：The ratio between the mole for changing AA and H2PdCl4, is prepared for AA:H2PdCl4=1 sample, and it is labeled as AA:Pd
=1.
Sample AA:The preparation process of Pd=1 is as follows:
It takes the AuNRs solution 2mL of CTAC modifieds to be placed in 40mL measuring cups, is diluted with water to 20mL；
It is firstly added 3mL0.01mol/L chloroplatinic acids and 4mL1mmol/L silver nitrates, it is anti-to add 600 μ L0.05mmol/L
Bad hematic acid stirs 30s at 700r/min, and then 30 DEG C of standing 12h, product centrifugal treating are washed twice, are finally dispersed in 5mL
In ultra-pure water.
Wherein, catalytic efficiency the following table 1 in embodiment.
Table 1：
| Catalyst property | Nano particle/nanometer | Catalytic rate | |
| AuNRs | 0 | 0.03 | |
| Embodiment one | AA:Pd=0.1 | 10.1 | 0.27 |
| Embodiment two | AA:Pd=0.25 | 14.5 | 0.31 |
| Embodiment three | AA:Pd=0.50 | 19.8 | 0.44 |
| Example IV | AA:Pd=1.00 | 31.5 | 0.29 |
The physical and chemical performance analysis of dumbbell shaped nanogold-platinum composite catalyst of the present invention is shown in attached drawing 1 and attached drawing 2.
Shown in Fig. 1, in the cyclic voltammetry curve figure of nitrogen and oxygen, in 0.1MKOH electrolyte, 100mVs-1Sweep speed.Current potential
Window -1.2~0.2V.Redox reaction has occurred between 0.2~-0.6.
Shown in Fig. 2, in the LSV curve graphs under nitrogen and oxygen different rotating speeds, in 0.1MKOH electrolyte, 10mVs-1Sweep speed.
As seen from the figure, it is 0.8V, half wave potential about 0.6V to play spike potential.Carrying current is under 2500RPM rotating speeds, about 1.8mAcm-2, illustrate that the application has preferable oxygen reduction catalytic activity.
Although the embodiments of the present invention has been shown and described above, it is to be understood that above-described embodiment is example
Property, it is not considered as limiting the invention, those skilled in the art are not departing from the principle of the present invention and objective
In the case of can make changes, modifications, alterations, and variations to the above described embodiments within the scope of the invention, it is carried out simply
Combination variation be all classified as the present invention protection within.
Claims (7)
1. a kind of dumbbell shaped nanogold-platinum composite catalyst, it is characterised in that：Including cetyl chloride ammonium, enuatrol, chlorine platinum
Acid, sodium borohydride, cetyl ammonium bromide, three hydration gold chlorides, silver nitrate, ascorbic acid, concentrated hydrochloric acid and concentrated nitric acid.
2. dumbbell shaped nanogold-platinum composite catalyst according to claim 1, it is characterised in that：The each component concentration
It is as follows
CTAC97%
NaOL97%
H2PtCl6·6H2O98%
NaBH499%
CTAB98%
HAuCl4·3H2O99.99%
AgNO399.99%
AA>99.5%
HCl36.0~37.0%
HNO365.0~68.0%.
3. a kind of preparation method of dumbbell shaped nanogold-platinum composite catalyst described in claim 1, it is characterised in that：Including
Following steps：
S1：Glass reaction container is impregnated into 12h in chloroazotic acid；
S2：CTAB is added in measuring cup, HAuCl is then added410~20min of solution ＆ stir is added freshly prepared
NaBH4Solution is vigorously stirred 2min, and solution colour becomes brown color from yellow, spare after standing 30min under the conditions of 30 DEG C；
S3：Weigh CTAB7.0g, NaOL1.234g, H2PtCl6·6H2O1.2g is placed in 500mL conical flasks, and is added
250mL55 DEG C of ultra-pure water waits for that solution is cooled to 30 DEG C, AgNO3 solution is added, and stand 15min under the conditions of 30 DEG C；Then
HAuCl is added4Solution, stirs 90min at 700r/min, and solution is become colorless by yellow；HCl is added, is stirred in 400r/min
Mix 15min；Then ascorbic acid is added in the mixed solution and is vigorously stirred 30s；0.4mL seed-solutions are finally taken to be added
Into growth solution, after being vigorously stirred 30s, 30 DEG C of standing 12h obtain gold nanorods stoste, the centrifugation of gold nanorods stoste and water
It washes twice, gained gold nanorods are dispersed in 0.1mol/L50mLCTAC solution, are stored in spare in 35 DEG C of baking oven；
S4：It is AA to adjust the ratio between mole of AA and H2PdCl4:Pd=0.5 prepares catalyst.
4. the preparation method of dumbbell shaped nanogold-platinum composite catalyst according to claim 3, it is characterised in that：In S4
Preparation process is as follows:
It takes the AuNRs solution 2mL of CTAC modifieds to be placed in 40mL measuring cups, is diluted with water to 20mL；
It is firstly added 3mL0.01mol/L chloroplatinic acids and 4mL1mmol/L silver nitrates, adds 300 μ L0.05mmol/L Vitamin Cs
Acid stirs 30s at 700r/min, and then 30 DEG C of standing 12h, product centrifugal treating are washed twice, and it is ultrapure to be finally dispersed in 5mL
In water, milkiness liquid catalyst is obtained.
5. the preparation method of dumbbell shaped nanogold-platinum composite catalyst according to claim 3, it is characterised in that：In S1
It is 3 that the chloroazotic acid, which is concentrated hydrochloric acid with concentrated nitric acid according to volume ratio,:The solution of 1 composition.
6. the preparation method of dumbbell shaped nanogold-platinum composite catalyst according to claim 3, it is characterised in that：In S2
The CTAB amounts are 0.2mol/L, 5mL；HAuCl4Solution is 0.5mmol/L, 5mL；NaBH4Solution is 6mmol/L, 1mL.
7. the preparation method of dumbbell shaped nanogold-platinum composite catalyst according to claim 3, it is characterised in that：In S3
The AgNO3 solution is 4mmol/L, 24mL；HAuCl4Solution is 1mmol/L, 250mL；HCl amounts are 37wt%, 4.8mL；
Ascorbic acid is 64mmol/L, 1.25mL.
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| CN112756623A (en) * | 2020-12-31 | 2021-05-07 | 杭州电子科技大学 | Synthesis method of gold-platinum material with special structure |
| CN112809018A (en) * | 2020-12-31 | 2021-05-18 | 杭州电子科技大学 | Synthesis method of gold-platinum bimetallic structure material |
| CN113385687A (en) * | 2021-06-11 | 2021-09-14 | 杭州电子科技大学 | Asymmetric gold-silver-platinum-silver multilayer composite material and synthetic method thereof |
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